Author's Accepted Manuscript

Parametric study of abrasive wear of Co-CrC

based flame sprayed coatings by Response
Surface Methodology
Satpal Sharma
PII: S0301-679X(14)00091-7
DOI: http://dx.doi.org/10.1016/j.triboint.2014.03.004
Reference: JTRI3274
To appear in: Tribology International
Received date: 14 January 2014
Accepted date: 4 March 2014
Cite this article as: Satpal Sharma, Parametric study of abrasive wear of Co-CrC
based flame sprayed coatings by Response Surface Methodology, Tribology
International, http://dx.doi.org/10.1016/j.triboint.2014.03.004
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1

Parametric study of abrasive wear of Co-CrC based flame sprayed coatings by
Response Surface Methodology
Satpal Sharma
School of Engineering, Gautam Buddha University, Greater Noida, U.P. (India)
E-mail-satpal78sharma@gmail.com
Abstract
Co base powder (EWAC1006 EE) was modified with the addition of 20%WC and the same was
further modified by varying amounts of chromium carbide (0, 10 and 20wt.%) in order to develop three
different coatings. Microstructure, elemental mapping XRD, porosity and hardness analysis of the three
coatings was carried out. The effect of CrC concentration (C), load (L), abrasive size (A), sliding distance
(S) and temperature (T) on abrasive wear of these flame sprayed coatings was investigated by response
surface methodology and an abrasive wear model was developed. A comparison of modeled and
experimental results showed 5-9 % error.
Keywords: Coating; Abrasive wear; Microhardness; Response Surface Methodology (RSM).
1 . Introduction
The progressive deterioration of metallic surfaces due to various types of wear (abrasive, erosive,
adhesive, corrosive and chemical wear) in various industries (coal and hydro thermal power plants,
cement, automotive, chemical and cement industry) leads to loss of plant operating efficiency and
frequent breakdown of the components which in turn results in huge financial losses to the industry. The
recognition of this fact has been the driving force behind the continuing development of the surface
modification and surface coating technologies known as surface engineering. The properties of these
surface layers may be different from those of the material as dictated by service requirements.
The cobalt base alloys have found a wide variety of tribological applications for abrasive and
adhesive wear resistance in many industries such as aerospace, automotive, hydro and gas turbines and
cement industry. Some studies [1-6] report the effect of processing techniques, carbide additions and their
2

distribution and post spray heat treatment on the hardness and abrasive wear resistance of Co base
coatings. The abrasive wear is influenced by a number of different factors such as the properties of the
materials (microstructure and hardness), the service conditions (applied load and abrasive grit size) and
environment (temperature and humidity). High hardness and good resistance to abrasion of cobalt based
coatings are generally attributed to the presence of high volume fraction of carbides. Increase in hardness
of these alloys with the addition of WC and TiC has been reported [7-8]
.
Maiti et al. [9] reported that with
addition of WC upto 20% in WC-Co-Cr coatings the increases the hardness and abrasive wear rsistance
and further addition of WC increases hardness marginally. In the present study, the Co base alloy was
modified with WC and varying amount of CrC

additions (0, 10 and 20%) to increase the hardness and
abrasive wear resistance of coatings.
In cement industry, various fans are used to transport alumina and silica particles of 5-50 micron
size along with hot gases (temperature 393-423K). These solid particles travel along the fan blade surface
at a very low angle (<10). Abrasive wear has been reported to simulate the low angle solid particle
erosion conditions [10-13]. Cement industry is trying many types of coating materials including cobalt
base alloy. Therefore, in this work a cobalt base alloy was selected for study and further developed for
improved abrasion and erosion performance. It has also been found from the literature that most of the
research on abrasive wear behavior of Co base alloys was carried out considering single dimensional
aspect of applied wear conditions such as abrasive grit size and load only. Data generated using
traditional method of research using single factor effect is valuable and detailed, but fails to indicate the
effect of their interactions of various test parameters on abrasive wear. Therefore, a number of statistical
methods have recently been implemented in wear studies. These methods share the advantage of
facilitating research into the effects of different factors and their interactions (combined effect), by
limiting the number of tests. Hence in this study an attempt has been made to study the independent as
well as combined effect of the factors using fractional factorial design (Response Surface Methodology).
Based on the experimental data obtained an abrasive wear model was developed to correlate the abrasive
wear of the coatings in terms of applied factors and their interactions. The validity of the abrasive wear
3

model was evaluated under different abrasive wear conditions by comparing the experimental and
modeled results.

2. Experimental procedure
2.1 Materials and methods
The carbon steel substrate was used for deposition of modified Co base alloy coatings. The
substrate was degreased and roughened to an average surface roughness of Ra 3.15 m (Rmax 18.2 m).
Surface roughness was measured by Mahr Perthometer (M
2
409). The nominal composition of substrate
and commercially available Co base powder (EWAC 1006 EE) is shown in Table 1. This powder was
modified by adding 20wt.% WC. Further addition of 0, 10 and 20wt.% CrC was carried out to develop
three different compositions ((1006EE + 20wt.% WC+ 0wt.% CrC), (1006EE + 20wt.% WC+ 10wt.%
CrC) and (1006EE + 20wt.% WC+ 20wt.% CrC)). In following sections these modified compositions are
designated by 0, 10 and 20wt.% CrC coatings respectively. These compositions were deposited using
flame spraying process by Super Jet spray torch (L & T India). The flame spraying was carried out using
neutral flame of oxy-acetylene gas where the pressures of oxygen and acetylene were maintained at 0.3
MPa (3kgf/cm
2
) and 0.12 MPa (1.2 kgf/cm
2
) respectively. The substrate was preheated to 20010
o
C. The
spraying parameters are shown in Table 2.
2.2 Characterization of coatings
Coated samples were cut transversely for microstructural characterization (SEM, SEM- LEO 435-
VP, England), porosity and hardness. The samples were polished using standard metallographic
procedure and etched with a chemical mixture of 3 parts HCl + 1 part HNO
3
. SEM micrographs were
used to study microstructure and worn surfaces. The porosity was measured by the point counting method
[14-20]. The average of 25 areas of each coating has been used for porosity measurement. Vickers
hardness of the coating was measured using a load of 5 kg and average of six readings of the coating was
used for study purpose. Scanning electron microscopy of the worn surfaces of coatings was also carried
out to identify the material removal mechanisms under abrasive wear conditions.
4

2.3 Factorial design of experiment
The vast amounts of data have been generated by the traditional approach of experiment design in
which one factor is varied at a time (load and abrasive grit size). In this approach it is difficult to evaluate
the combined effects of applied factors. This is the main reason why load has always been considered first
in wear research, whilst other factors, e.g. abrasive grain size, sliding distance and their combined effects
(load and abrasive size, load and speed, abrasive size and sliding distance), which may also be important,
have not been given the attention they deserve. The advantage of the statistical method is obvious [12].
Thus RSM (Response Surface Methodology) with fractional factorial design of experiments with three
levels of each factor has been used in the present study. According to Rabinowiczs classic theory [21]
that claims applied load and hardness (depends upon composition) of materials are the most important
factors affecting the abrasion process, therefore, both these factors were considered along with the
abrasive size and sliding distance in this study. Temperature is also taken as fifth factor in this study.
Thus five factors composition, load, abrasive size, sliding distance and temperature were used in the
present study. These factors were designated as C (composition- % CrC concentration), L (load-N), A
(abrasive size-m), sliding distance(S) and temperature (T) respectively. The coded value of upper,
middle and lower level of the three factors is designated by +1, 0 and -1 respectively. The actual and
coded values (in parentheses) of various factors used in the present study are shown in Table 3. The
experimental design matrix for different runs is shown in Table 4. The relation between the actual and
coded value of a factor is shown below:
2 /


conditions test of Range
conditions test Mean conditions test Actual
value Coded

2.4 Wear test
Wear behavior of flame sprayed coatings (0, 10 and 20wt.% CrC) was studied using pin on disc
type wear testing unit. Coated wear pins of size 5535 mm were held against abrasive medium under
different runs. Water proof SiC abrasive papers were used as abrasive medium. Abrasive paper was
mounted on a steel disc (21020 mm), which was rotated at 2004, 2965 and 3685 rpm (revolution per
5

minute) corresponding to the sliding distance of 25, 55 and 85 m. The slide carrying the wear pin was
moved radially to get the spiral motion under a constant increment of 0.2 mm of the wear pin. The
abrasive wear pin and disc carrying the abrasive paper was enclosed in a heating chamber. Three
thermocouples were used for measuring the temperature of the heating chamber. The test temperature was
controlled with the temperature controller unit (target temperature 5C). The tester was allowed to run
idle for 2 minute in order to attain the constant rpm (without reciprocating motion); afterwards load was
applied and simultaneously the reciprocating unit was switched on to have a spiral motion of the wear pin.
Wear tests were conducted randomly according to design matrix (Table 4) under different runs and two
replications under each run were taken and average value of abrasive wear has been reported in Table 4.
An electronic Mettler micro balance (accuracy 0.0001 g) was used for weighing the samples after
washing in acetone before and after abrasive wear. Weight loss was used as a measure of abrasive wear
(g).

3 Results and discussion
3.1 Microstructure
The microstructures and EDAX analysis of 0wt.% chromium carbide, 10wt.% chromium carbide
(not shown for brevity) and 20wt.% chromium carbide coatings are shown in Figs. 1 (a-d) - 2 (a-d)
respectively. The microstructures were taken from the center region of the coatings. All the three coatings
mainly showed eutectic (A), W dominated carbides (B) and Cr dominated carbides (C).
The eutectic A is found to be composed of Co, Ni, Fe and Cr with small amount of W and C.
EDAX analysis of eutectic showed 30% Co, 24% Ni and 15% Fe (wt%) and other elements such as
8%Cr, 6%W, 5%C (wt%) (average of 6 readings in each case has been reported) (Fig. 1b). The W
dominated carbides B and Cr dominated carbides C are present in the eutectic matrix A. These W
and Cr dominated carbide particles primarily differ in terms of relative amounts of various elements such
as W, Cr and Co etc. The EDAX analysis of W dominated carbides showed 57%W, a10% Co, a10% Cr
and a10% Ni and 4%C (wt.%) (Fig. 1c). The Cr dominated carbides C are rich in Cr and contain
6

52%Cr, 15%W, 13%Co, 7%C besides small amounts of Ni and Fe (<5%) (wt.%) as shown by the EDAX
analysis (Fig. 1d).
The microstructures and EDAX analysis of 10wt.% chromium carbide (not shown fro brevity) and
20wt.% chromium carbide coatings are shown in Fig. 2 (a-d). Both these chromium carbide modified
coatings exhibited features similar to that of 0wt.% chromium carbide coating except that compositions of
eutectic and carbides were different. The quantitative EDAX analysis showed that the wt.% of Co (|30
wt.%) is same in the eutectic matrix of all the three coatings (0wt.% chromium carbide, 10wt.%
chromium carbide and 20wt.% chromium carbide) and it is uniformly distributed in the eutectic matrix as
shown in elemental maps (Fig. 3 a-2, b-2 and c-2). These results are in agreement with findings of Shetty
et al. [22] as they reported that the eutectic matrix is rich in Co containing various types of carbides,
which are uniformly distributed in the matrix. The other elements such as Ni, Fe and Cr are also
uniformly distributed in the eutectic matrix (Fig. 3 a-c). However, wt.% of Cr increased from 8-14 wt.%
with the addition of chromium carbide. Some of the carbide particles appear darker in SEM micrographs
as can be seen in Fig. 1, and 2. This observation is also in line with the findings of Shetty et al. [22].
Image analyses of three coatings viz. 0wt.% chromium carbide, 10wt.% chromium carbide and
20wt.% chromium carbide was carried out to determine the volume fraction of eutectic, W dominated and
Cr dominated carbides (A, B and C respectively). The volume fraction of eutectic A was found
as 72.1%, 65.7% and 46.1% respectively in 0% chromium carbide, 10% chromium carbide and 20%
chromium carbide coatings respectively. The volume fraction of W dominated carbides B was found as
13.8%, 17% and 27.5% respectively, whereas the Cr dominated carbides C was observed as 14.1%,
18.3% and 26.4% respectively in the three coatings (0wt.% chromium carbide, 10wt.% chromium carbide
and 20wt.% chromium carbide).

3.2 XRD analysis
XRD analysis of 0 wt.% chromium carbide coating (Fig. 4) mainly showed Ni- Cr-Fe-C, M
23
C
6

(M=Ni, Cr, Co, Fe), CoWSi, Ni
4
W and Fe
3
C phases in the coating. Cr
23
C
6
as main carbides was found to
7

be present in the 10wt.% chromium carbide coating (Fig. 5) besides small amount of Cr
7
C
3,
FeNi
3
and
Ni
31
Si
12
were also observed in 10wt.% chromium carbide coating. Cr
7
C
3
as the main carbides was found
in the 20wt.% chromium carbide coating besides Co
3
W
9
C
4,
FeNi
3
and Co
7
W
6
phases (Fig. 6). These
finding are in agreement with the published literature [23- 27]. With the addition 10wt.% and 20wt.%
chromium carbide, the carbides types were changed from M
23
C
6
to Cr
23
C
6
and Cr
7
C
3
and some
intemetallic compounds (Co
7
W
6
and Co
3
W
9
C
4
) also formed.
The various types of carbides (M
23
C
6,
Cr
3
C
2
and Cr
7
C
3
) are not pure phases but also contain Ni,
Co, Cr and Fe as revealed by the elemental mapping (Fig. 3 c-1 to c-5) of the various coatings, where Ni,
Co, Cr and Fe are also present in these phases of coatings. As shown by marked circle area C in Fig. 3
c-1, c-3 and c-6, this region may correspond to chromium carbide (Cr
7
C
3
as detected by XRD analysis
(Fig. 6). This area C also contains Co, Ni and Fe as shown in Fig. 3 c-2, c-4 and c-5 respectively. Thus,
it is inferred that these carbides are not pure phases. These results are in agreement with the findings of
Chorcia et al. [27].
3.3 Hardness and porosity
The Vickers hardness (Hv
5
) and porosity (%) of the three coatings with varying wt.% of
chromium carbide (0 wt.% chromium carbide, 10 wt.% chromium carbide and 20wt.% chromium
carbide) are shown in Fig. 7 (a) and (b) respectively. Vickers hardness of three coatings was measured
using a normal load of 5kg and average value of six readings of hardness of the coating cross-section has
been used for study. The average Vickers hardness (Hv
5
) of three coatings (0 wt.% chromium carbide, 10
wt.% chromium carbide and 20 wt.% chromium carbide) was found to be

69686 Hv
5
, 74195 Hv
5
and
786112 Hv
5
respectively (Fig 7a). The average hardness of 20wt.% chromium carbide coating was
found higher (786 Hv
5
) as compared to 0 wt.% chromium carbide (696 Hv
5
) and 10 wt.% chromium
carbide (741 Hv
5
) coatings, however, there was a more scatter in hardness of 20 wt.% chromium carbide
coating as compared to 0 wt.% chromium carbide and 10% chromium carbide coatings may be due to
higher porosity (Fig. 7b).

8

The higher hardness of 10 wt.% chromium carbide coating as compared to 0 wt.% chromium
carbide is due to formation of Cr
23
C
6
carbides and intemetallic compound Co
7
W
6
as detected by XRD
analysis (Fig. 5). The highest hardness of 20 wt.% chromium carbide coating as compared to other two (0
wt.% chromium carbide and 10 wt.% chromium carbide) is mainly due to formation of Cr
7
C
3
carbides as
detected by XRD analysis (Fig. 6). The formation of Cr
7
C
3
and Cr
23
C
6
carbides increases the hardness of
the coating owing to their high hardness. The hardness of Cr
7
C
3
and Cr
23
C
6
is 17.7 GPa and 9.9 GPa
respectively as reported by Lebaili et al. [28]. It has also been reported [24, 25] that some of the
chromium may be replaced by cobalt and/or tungsten with a matrix of eutectic containing the other
constituents of the alloy, thus forming intermetallic compounds. In this investigation also it has been
observed that Co
7
W
6
and Co
3
W
9
C
4
intermetallic compounds were formed as found in the XRD analysis
of 10 wt.% chromium carbide and 20 wt.% chromium carbide coating (Fig. 5, 6). Otterloo et al. [24, 25]
reported that the intermetallic compounds (Co
7
W
6
and Co
3
W
9
C
4
) also increase the hardness of Co-base
alloys. Thus, the higher hardness of 10 wt.% chromium carbide and 20 wt.% chromium carbide coatings
can also be attributed to formation of these intermetallic compounds as detected by XRD analysis (Fig. 5,
6). The porosity of all the three coatings was found to be 7.7%, 8.6% and 9.2% respectively (Fig. 7b).

3.4 Abrasive wear model
In the present work RSM was applied for developing the mathematical models in the form of
multiple regression equations for the abrasive wear. In applying the RSM the dependent variable
(abrasive wear) is viewed as a surface to which the model is fitted. Evaluation of the parametric effects on
the response (abrasive wear) was done by considering a second order polynomial response surface
mathematical model given by:

r
j i
k
i
k
i j
ij i ii
k
i
i
k
i
i
x x b x b x b b Wr H

1
1 1
2
1 1
0
(1)
This equation of abrasive wear (assumed surface) Wr contains linear, squared and cross product
terms of variable x
i
s (C, L, A, S and T). b
0
is the mean response over all the test conditions (intercept), bi
9

is the slope or linear effect of the input factor x
i
(the first-order model coefficients), bii the quadratic
coefficients for the variable i (linear by linear interaction effect between the input factor x
i
and x
i
) and bij
is the linear model coefficient for the interaction between factor i and j. The face centered composite
design was used in this experimental study. Significance testing of the coefficients, adequacy of the
model and analysis of variance was carried out to using Design Expert Software to find out the significant
factors, square terms and interactions affecting the response (abrasive and erosive wear).
R
is the
experimental error.
The analysis of variance (ANOVA) is shown in Table 5. The analysis of variance (ANOVA)
shows the significance of various factors and their interactions at 95% confidence interval. ANOVA
shows the Model as Significant while the Lack of fit is Not significant which are desirable from
a model point of view. The probability values < 0.05 in the Prob.>F column indicates the significant
factors and interactions. The main factors and their interactions are included in the final abrasive wear
model while the insignificant interactions are excluded from the abrasive wear model. Composition (C),
load (L), abrasive size (A) and sliding distance (S) are the significant factors while composition-load
(CL), composition-temperature (CT), load-abrasive size (LA), load-sliding distance (LS) and abrasive
size-sliding distance (AS) are the significant interactions. The abrasive wear model generated in terms of
coded and actual factor values (equation 2 and 3 respectively) is given below:


Wr =0.015 - 4.86 10
-3
C + 0.013 L + 9.73 10
-3
A + 0.016 S 2.3310
-4
T + 9.9510
-3
S
2
-3.310
-3
CL
+ 4.2710
-3
CT + 5.4510
-3
LA + 8.1310
-3
LS + 8.42 10
-3
AS
R
(2)

Wr =0.053 8.46 10
-4
C -7.19 10
-4
L 3.47 10
-4
A 1.5210
-3
S 9.02 10
-5
T + 1.1110
-5
S
2
-
3.310
-5
CL + 8.5510
-6
CT + 1.3610
-5
LA + 2.7110
-5
LS + 7.02 10
-6
AS
R
(3)

3.5 Validity of the abrasive wear model
The validity of the abrasive wear model was evaluated by conducting abrasive wear tests on
coatings at different values of the experimental factors such as applied load (L), abrasive sizes (A), sliding
10

distance(S) and temperature (T). The actual and coded value of various factors for confirmation tests are
shown in Table 6. The variations between the experimental and the calculated values are of the order of
59%.
3.6 Effect of individual variables on wear rate
The effect of individual factors on abrasive wear is shown in Fig. 8 (a-e). The effect of
composition (C), load (L), abrasive size (A), sliding distance(S) and temperature (T) and that of their
interactions on abrasive wear are given in equation (2) which exhibits the abrasive wear in terms of coded
value and equation (3) in terms of actual values of factors and their interactions. However, the effects of
individual factors are discussed by considering the equation (2) because all the factors are at the same
level (+1, 0 and -1). The constant 0.015 in the equation (2) indicates the overall mean of the abrasive wear
of coatings under all the test conditions. This equation further indicates that the coefficient (-4.8610
-3
)
associated with composition (%CrC

concentration) is negative, which signifies a decrease of abrasive
wear with an increase of CrC concentration (Fig. 8 a). This is attributed to the increase in hardness of the
coating with increasing CrC concentration. Increase in hardness of material lowers the depth of
penetration of abrasive particles, therefore, results in shallow and finer wear grooves and reduced volume
of material removed. The effect of load, abrasive size, sliding distance and temperature on abrasive wear
is shown in Fig. 8 (b-e). The coefficient associated with load, abrasive size, sliding distance and
temperature are 0.013, 9.7310
-3
0.016 and -2.3310
-4
respectively. This signifies that sliding distance has
a more detrimental effect than the applied load on the abrasive wear of the coating. This is due to the fact
that the load determines the depth of penetration of abrasive in the material whereas there is a prolonged
interaction of abrasives at higher sliding distances. Thus, for the same load the abrasive wear increases
with the increase in sliding distance as shown in Fig. 8d. The effect of abrasive size on the wear is less as
compared to sliding distance and load. The abrasive wear increases with the increase in abrasive size (Fig.
8) as there is a greater tendency for large penetration of sharp abrasives with the increase of abrasive size,
attributed to increase in actual contact area and hence the effective load [12]. This leads to deeper and
wider grooves and finally causes more severe wear of the coating. The penetration of the small size
11

abrasives is limited to its height of projection in the specimen surface. Thus the depth of penetration is
reduced even with the increase in load on small abrasive sizes which results in reduced wear of coatings.
The reduction in abrasive wear at higher temperature may be due to removal of some abrasive particles
from the abrasive paper.
3.7 Interaction effect of the different variables
The coefficients associated with the interaction terms CL (composition-load), CT (composition-
temperature), LA (load-abrasive size), LS (load-sliding distance) and AS (abrasive size-sliding distance)
in equation (2) are -3.310
-3
, 4.2710
-3
, 5.4510
-3
, 8.1310
-3
and 8.42 10
-3
respectively showed the
extent of interaction (combined) effect of different factors on abrasive wear of coatings. The effect of
interactions among the different factors on abrasive wear is almost same order as of their individual
effects. The combined effect of composition -load (CL) is the lowest from all significant interactions.
The combined effect of various abrasive wear test parameters on the wear behavior of coatings
has been shown in the form of response surface plots (Fig. 9 a-e). The combined effect of CL
(composition-load) interaction can be explained by considering equation 2 and Fig. 9 (a). The ve sign
associated with the coefficient of CL interaction shows the reduction in wear of the coating. The Fig.9 (a)
shows that the abrasive wear increases with the increase in load due to more penetration effect of abrasive
in the coating while the wear reduces due to increase of CrC concentration from 0 to 20wt.%. The
reduction in wear at high CrC concentration is due to increase in hardens of coating. The overall effect of
CL interaction is to reduce the wear of the coating. The CT (composition-temperature) interaction can be
explained on similar lines by considering equation 2 and Fig. 9 (b).
The combined effect of load and abrasive size (LA) on wear of coatings shows that the wear of
coatings increases with an increase in both the load and abrasive size. Moreover, the effect of increase in
load at high abrasive size is more predominant than at low abrasive size. Further, it can be observed from
response surface plot that the effect of increase in abrasive size on wear of coatings is more at high loads
than at low loads. This is attributed to the fact that at high load and large abrasive size, the depth of
12

penetration of abrasive increases. This leads to more abrasive wear at high load and high abrasive size and
vice versa.
The combined effect of load-sliding distance (LS) on wear of coatings shows that the wear of
coatings increases with an increase in both the load and sliding distance. Moreover, the effect of increase
in sliding distance is more predominant than the increase in load on abrasive wear. However, the effect of
increase in sliding distance is more predominant in the entire range of loading on abrasive wear as
compared to increase in load. Further, it can be observed from response surface plot that the effect of
increase in sliding distance on wear of coatings is more at high loads than at low loads.
The combined effect of abrasive size and sliding distance (AS) on wear of coatings shows that the
wear of coatings increases with an increase in both the sliding distance and abrasive size. Again the effect
of increase in sliding distance on abrasive wear is more predominant in the entire range of abrasive size. It
can be observed from response surface plot that the effect of increase in sliding distance on wear of
coatings is more at high abrasive size than at low abrasive size. Thus high abrasive size and high sliding
distance results in severe wear of the coatings. Same effects of load, abrasive size and sliding distance
were observed in LS and AS interactions for abrasive wear of coatings as discussed above.
3.8 SEM study of worn surfaces
In an attempt to identify the abrasive wear mechanism in 0, 10 and 20% CrC coatings; SEM
images of worn surfaces were analyzed (Fig.10 a-b). The worn surfaces of various coatings (0, 10 and
20wt.% CrC) mainly showed the ploughing and cutting mechanisms (Fig. 10 a-b). The weight loss in
each coating is determined by the extent of these mechanisms. Ploughing and cutting mechanism were
observed in the 0% CrC coating

while cutting mechanisms were observed in 10 and 20%CrC coatings.
The worn grooves are wider in 0 and 10% CrC coatings as compared to 20% CrC coating. The wider
grooves in 0% CrC and 10% CrC coating were due to low hardness as compared to 20% CrC coating.
Due to sharp abrasive particles the width of the cutting/ ploughing grooves increases with the increase in
depth of indentation and results in increase in wear rate of the coatings.
13

The chromium carbide concentration increases the wear resistance of the coatings. Experimental
and confirmation test results showed that the weight loss in 20% CrC coating is lowest. The weight loss
of 20% chromium carbide coating is 1.5 times lower as compared to 0% chromium carbide coating. This
is attributed to higher hardness of the coating.
4 Conclusions
The following conclusions can be drawn from the present study:
1. The hardness increases with the increases in chromium carbide concentration. The maximum hardness
was obtained with 20wt.% chromium carbide. The increase in hardness is due to formation of new
phases and inetrmetallic compounds.
2. Response Surface Methodology (RSM) with fractional factorial design approach is an excellent tool,
which can be successfully used to develop an empirical equation for the prediction and understanding
of wear behavior of coatings in terms of individual factors (C, L, A, S and T) as well as in terms of the
combined effects (CL, CT, LA, LS and AS) of various factors.
3. The load and sliding distance has a more severe effect on abrasive wear of the coating as compared to
abrasive size.
4. Interactions effects of various factors on abrasive wear is almost of same order less than their main
factor effects. The interaction effect of abrasive size-sliding distance (AS) is considerably higher than
load-abrasive size (LA). Increasing (%) CrC concentration; reducing load, abrasive size and sliding
distance minimize the abrasive wear significantly.
5. Increase in chromium carbide concentration increases the abrasive wear resistance of the coatings.
Abrasive wear rate of 20wt.% chromium carbide coating is lower as compared to 0wt.% chromium
carbide coatings.

References:
[1] Desai V. M., Rao C. M, Kosel T. H. and Fiore N. F., Effect of carbide size on the abrasion of cobalt-
base powder metallurgy alloys, Wear 1984; 94: 89-101.
14

[2] Shetty H. R., Kosel T. H. and Fiore N. F., A study of abrasive wear mechanisms in cobalt-base alloys,
Wear 1983; 84:327-343.
[3] Kim H. J. and Kim Y. J., Wear and corrosion resistance of PTA weld surfaced Ni and CO based alloy
layers, Surface Engineering, 1999; 15(6): 495-501.
[4] Atamert, S and Bhadesia H. K. D. H., Comparison of the microstructures and abrasive wear properties
of stellite hardfacing alloy deposited by arc welding and laser cladding, Metallurgical Transactions A
(Physical Metallurgy and Materials Science), 1989; 20A: 1037-54.
[5] Yadav A.K., Arora N., and Dwivedi D. K., On microstructure, hardness and wear behavior of flame
sprayed Co base alloy coating deposited on mild steel, Surface Engineering, 2006; 22: 331-6.
[6] Hrasha S. and Dwivedi D. K., Microstructure, hardness and abrasive wear behavior of flame sprayed
Co based alloy coatings, Surface Engineering, 2007; 23(4): 1-6.
[7] Harsha S., Dwivedi D. K., Agrawal A., Influence of WC addition in CoCrWNiC flame sprayed
coatings on microstructure, microhardness and wear behavior, Surf & Coat Technol, 2007; 201:
576675.
[8] Nishida, Minoru, Effect of TiC-Cr
3
C
2
particles content on abrasive wear resistance of Co-base overlay
weld alloy, Journal of the Japan Welding Society,1993; 11: 156-61.
[9] Maiti A.K., Mukhopadhyay N., Raman R., Effect of adding WC powder to the feedstock of WCCo
Cr based HVOF coating and its impact on erosion and abrasion resistance, Surf & Coat Technol,
2007; 201: 778188.
[10] Fernndez J. Esteban, Fernndez Ma del Rocio, Diaz R. Vijande, Navarro R. Tucho, Abrasive wear
analysis using factorial experiment design, Wear 2003;255: 3843.
[11] Hejwowski T., Szewczyk S., Weronaski A., An investigation of the abrasive and erosive wear of
flame-sprayed coatings, J Materials Process Technol 2000; 106: 54-7.
[12] Venkateswarlu K., Mohapatra S., Rao R.G., Ray A.K., Pathak L.C. and Mondal D.P., High abrasive
wear response of diamond reinforced composite coating: a factorial design approach, Tribology
Letters, 2006; 24: 7-14.
15

[13] Spuzic S., Zec M., Abhary K., Ghomashchi R., Reid I., Fractional design of experiments applied to a
wear simulation, Wear 1997; 212: 1319.
[14] Sharma S.P., Dwivedi D.K. and Jain P.K., Effect of CeO
2
addition on the microstructure, hardness,
and abrasive wear behavior of flame-sprayed Ni-based Coatings. Proceedings of the Institution of
Mechanical Engineering, Part J- Journal of Engineering Tribology, 2008; 222: 925-33.
[15] Sharma S.P., Dwivedi D.K. and Jain P.K., Effect of La
2
O
3
addition on the microstructure, hardness
and abrasive wear behavior of flame sprayed Ni based coatings. Wear 2009; 267: 853-9.
[16] Kim Hyung-Jun, Yoon Byoung-Hyun, Lee Chang-Hee, Sliding wear performance in molten ZnAl
bath of cobalt-based overlays produced by plasma-transferred arc weld-surfacing Wear 2003; 254:
408-14.
[17] ASTM standards E 2109 01. Standard Test Methods for Determining Area Percentage Porosity in
Thermal Sprayed Coatings, (Reapproved 2007).
[18] ASTM standards E 562 05e1. Standard Test Method for Determining Volume Fraction by
Systematic Manual Point Count.
[19] Hidalgo V. Higuera, Varela F.J. Belzunce, Menendez A. Carriles, Martnez S. Poveda, A
comparative study of high-temperature erosion wear of plasmasprayed NiCrBSiFe and WC
NiCrBSiFe coatings under simulated coal-fired boiler conditions, Tribology International 200; 34:
1619.
[20] Hidalgo V. Higuera, Varela J. Belzunce, Menndez A. Carriles, Martnez S. Poveda,
High temperature erosion wear of flame and plasma-sprayed nickelchromium coatings under
simulated coal-fired boiler atmospheres, Wear 2001; 247: 21422.
[21] Rabinowicz E.D., Friction and Wear of Work Hardening in the Design of Wear Resistant Materials,
Wiley, New York, 1965, p. 168.
[22] Shetty H. R., Kosel T. H. and Fiore N. F., A study of abrasive wear mechanisms using
diamond and alumina scratch tests, Wear 1982; 80: 347 76.
[23] Radu Iulian, Li D.Y., Llewellyn R., Tribological behavior of Stellite 21 modified with
16

yttrium, Wear 2004, 257: 1154 -66.
[24] Otterloo J. L. De Mol Van and Hossont J. TH. M. De, Microstructure and Abrasive Wear
of Cobalt-Based Laser Coatings, Scripta Materialia 1997; 36: 239- 45.
[25] Otterloo J. L. De Mol Van and Hossont J. TH. M. De, Microstructural features and
mechanical properties of a cobalt - based laser coating, Acta materialia 1997;
45:1225-36.
[26] Shin Jong-Choul, Doh Jung-Man, Yoon Jin-Kook, Lee Dok-Yol, Kim Jae-Soo, Effect of
molybdenum on the microstructure and wear resistance of cobalt-base Stellite
hardfacing alloys, Surf & Coat Technol,2003; 166: 11726.
[27] Corchia M., Delogu P. and Nenci F., Microstructural aspects of wear- resistant stellite and
colmonoy coatings by laser processing, Wear 1987; 119: 137-52.
[28] Lebaili S., Durand-Charee M., Hamar-Thibault S., The metallurgical structure of as
solidified Ni-Cr-B-Si-C hardfacing alloys, J Mat Sci, 1988; 23: 3603 11.
17



Table Captions

Table 1 Chemical composition (wt. %) of substrate and surfacing powder
Table 2 Flame spray parameters
Table 3 Various factors and their levels
Table 4 Design matrix and various factors with their actual and coded values (in parentheses)
Table 5 Analysis of variance (ANOVA)
Table 6 Confirmations test results

















18


Table 1 Chemical composition (wt. %) of substrate and surfacing powder
C Cr W Si Fe Co Mn
Substrate 0.2-0.22 _ _ 0.4-0.6 Balance _ 0.4-0.8
1006 EE Powder 3.0-3.5 28-30 5-6 0.2-0.5 _ Balance 0.5-0.7


Table 2 Flame spray parameters






Table 3 Various factors and their levels
Factor Designation Lower level Middle level Upper level
Composition, %wt.
CrC
C 0 (-1) 10 (0) 20 (+1)
Load, N L 5 (-1) 15 (0) 25 (+1)
Abrasive size,
m {grit size}
A 202* {500} (-
1)
60 4*{220} (0) 1005 *{120}
(+1)
Sliding distance, m S 25 (-1) 55 (0) 85 (+1)
Temperature, C T 50 (-1) 100 (0) 150 (+1)
* As given by manufacturer.


Table 4 Design matrix and various factors with their actual and coded values (in parentheses)
Run No. Composition
(C)
Load (L) Abrasive size
(A)
Sliding
distance(S)
Temperature
(T)
Av. wt..
loss (g)
1 0 (-1) 25 (+1) 20 (-1) 25 (-1) 50 (-1) 0.0179
Parameters Value
Vertical distance of spray nozzle from substrate 18 mm
Spraying speed 120 mm/ min.
Interior angle of spray nozzle with the horizontal 65
o

19

2 20 (+1) 25 (+1) 20 (-1) 85 (+1) 50 (-1) 0.0209
3 0(-1) 15 (0) 60 (0) 55 (0) 100 (0) 0.0146
4 10 (0) 25 (+1) 60 (0) 55 (0) 100 (0) 0.0215
5 10 (0) 15 (0) 100 (+1) 55 (0) 100 (0) 0.0172
6 0(-1) 25 (+1) 100 (+1) 85 (+1) 50 (-1) 0.104
7 10 (0) 15 (0) 20 (-1) 55 (0) 100 (0) 0.0061
8 10 (0) 5 (-1) 60 (0) 55 (0) 100 (0) 0.0066
9 20 (+1) 25 (+1) 100 (+1) 25 (-1) 50 (-1) 0.0151
10 10 (0) 15 (0) 60 (0) 55 (0) 150 (+1) 0.0144
11 20 (+1) 15 (0) 60 (0) 55 (0) 100 (0) 0.0147
12 10 (0) 15 (0) 60 (0) 55 (0) 100 (0) 0.0161
13 0(-1) 5 (-1) 100 (+1) 85 (+1) 150 (+1) 0.0338
14 20 (+1) 25 (+1) 20 (-1) 25 (-1) 150 (+1) 0.0057
15 20 (+1) 5 (-1) 20 (-1) 25 (-1) 50 (-1) 0.0028
16 0(-1) 25 (+1) 100 (+1) 25 (-1) 150 (+1) 0.0205
17 0(-1) 5 (-1) 20 (-1) 85 (+1) 50 (-1) 0.012
18 0(-1) 5 (-1) 20 (-1) 25 (-1) 150 (+1) 0.0051
19 10 (0) 15 (0) 60 (0) 25 (-1) 100 (0) 0.0048
20 0(-1) 25 (+1) 20 (-1) 85 (+1) 150 (+1) 0.0473
21 10 (0) 15 (0) 60 (0) 85 (+1) 100 (0) 0.0356
22 20 (+1) 5 (-1) 20 (-1) 85 (+1) 150 (+1) 0.0097
23 20 (+1) 25 (+1) 100 (+1) 85 (+1) 150 (+1) 0.0778
24 20 (+1) 5 (-1) 100 (+1) 85 (+1) 50(-1) 0.0237
25 20 (+1) 5 (-1) 100 (+1) 25 (-1) 150 (+1) 0.0039
26 10 (0) 15 (0) 60 (0) 55 (0) 50(-1) 0.0194
27 0(-1) 5 (-1) 100 (+1) 25 (-1) 50 (-1) 0.0066
28 10 (0) 15 (0) 60 (0) 55 (0) 100 (0) 0.0151
29 10 (0) 15 (0) 60 (0) 55 (0) 100 (0) 0.0188
30 10 (0) 15 (0) 60 (0) 55 (0) 100 (0) 0.0142



Table 5 Analysis of variance (ANOVA)
20


Source Sum
Squares
Degrees
Of
Freedom
Mean
Square
F
Value
Prob>F
Model 0.013 11 1.2110
-3
48.45 < 0.0001 Significant
Composition- C 4.2510
-4
1 4.2510
-4
17.10 0.0006
Load-L 2.85010
-3
1 2.85010
-3
114.58 < 0.0001
Abrasive size
A
1.70310
-3
1 1.70310
-3
68.48 < 0.0001
Sliding
distance- S
4.43110
-3
1 4.43110
-3
178.12 < 0.0001
Temperature -
T
9.80010
-7
1 9.80010
-7
0.039 0.8449
Interaction CL 1.74210
-4
1 1.74210
-4
7.00 0.0164
Interaction CT 2.9210
-4
1 2.9210
-4
11.76 0.0030
Interaction LA 4.75210
-4
1 4.75210
-4
19.11 0.0004
Interaction LS 1.05610
-3
1 1.05610
-3
42.46 < 0.0001
Interaction AS 1.13610
-3
1 1.13610
-3
45.66 < 0.0001
Residual error 4.47710
-4
18 2.48710
-5

Lack of fit 4.35810
-4
15 2.90610
-5
7.33 0.0632 Not
significant
Pure error 1.18910
-5
3 3.96310
-6





Table 6 Confirmations test results

21





Composition (C)
% CrC
Load
(L),
N
Abrasive
size(A) m
{grit size}
Sliding
distance
(S) m
Temperature
(T) C
Modeled
abrasive
wear (g)
Experimental
abrasive wear
(g)
%
Error
0 (-1) 15 (0) 422
{320}(-0.5)
70 (+0.5) 100 (+0.5) 0.0238 0.0250 4.8
10 (0) 15 (0) 422 {320}
(-0.5)
70 (+0.5) 100 (+0.5) 0.019 0.0173 8.95
20 (+1) 15 (0) 422 {320}
(-0.5)
70 (+0.5) 100 (+0.5) 0.0141 0.0152 7.24
22

Research Highlights
x The hardness increases with the increases in chromium carbide concentration.
x The load and sliding distance has more severe effect on abrasive wear of coating.
x Abrasive wear rate of 20wt.% chromium carbide coating is lower as compared to 0wt.%.


18

Figure Captions

Fig. 1 Microstructure and EDAX analysis of 0wt.% chromium carbide coating (a)
microstructure of coating, (b) EDAX analysis of eutectic, (c) EDAX analysis of
W dominated carbide and (d) EDAX analysis of Cr dominated carbide.
Fig. 2 Microstructure and EDAX analysis of 20wt.% chromium carbide coating (a)
microstructure of coating, (b) EDAX analysis of eutectic, (c) EDAX analysis of
W dominated carbide and (d) EDAX analysis of Cr dominated carbide.
Fig. 3 Elemental maps showing the distribution of Co, Cr, Ni, Fe, and C in (a) 0 wt.%
chromium carbide, (b) 10 wt.% chromium carbide and (c) 20 wt.% chromium
carbide coatings.
Fig. 4 XRD spectrum showing various phases in 0 wt.% chromium carbide coating.
Fig. 5 XRD spectrum showing various phases in 10 wt.% chromium carbide coating.
Fig. 6 XRD spectrum showing various phases in 20 wt.% chromium carbide coating.
Fig. 7 Effect of chromium carbide addition in 1006-20wt.%WC powder coating
on (a) hardness (Hv
5
) and (b) porosity (%).
Fig. 8 Effects of individual factors such as (a) %CrC-concentration, (b) load, (c) abrasive
size (d) sliding distance and (e) temperature on abrasive wear.
Fig. 9 Effects of interactions (a) composition load, (b) composition temperature, (c)
load- abrasive size, (d) load- sliding distance and (e) abrasive size and - sliding
distance on abrasive wear.
Fig. 10 SEM micrographs of worn surfaces (a) 0%wt. chromium carbide, (b) 10%wt.
chromium carbide and (c) 20%wt. chromium carbide.

19










Fig. 1 Microstructure and EDAX analysis of 0wt.% chromium carbide coating (a)
microstructure of coating, (b) EDAX analysis of eutectic, (c) EDAX analysis of
W dominated carbide and (d) EDAX analysis of Cr dominated carbide.
Eutectic A
c
b
d
W dominated
carbides B
Cr dominated
Carbides C
Cr dominated
Carbides C
Eutectic
A
W dominated
carbides B
a
Eutectic A
20


Fig. 2 Microstructure and EDAX analysis of 20wt.% chromium carbide coating (a)
microstructure of coating, (b) EDAX analysis of eutectic, (c) EDAX analysis of
W dominated carbide and (d) EDAX analysis of Cr dominated carbide.

a
Eutectic A
W dominated
carbides B
Cr dominated
Carbides C
c
b
d
Eutectic A
W dominated
carbides B
Cr dominated
Carbides C
2
1

(
a
)




































































(
b
)






























































(
c
)

F
i
g
.

3

C
o
n
t
i
n
u
e
d
.

C
o
C
o
C
o
3
a
-
1
3
a
-
2
3

b
-
2

3
c
-
2
3

b
-
1

3
c
-
1
A
r
e
a

A
r
e
a

2
2

(
a
)




































































(
b
)






























































(
c
)

F
i
g
.

3

C
o
n
t
i
n
u
e
d
.

C
r
N
i
C
r
C
r
N
i
N
i
3
a
-
3
3
a
-
4
3

b
-
4

3
c
-
4
3

b
-
3

3
c
-
3
A
r
e
a

A
r
e
a

2
3
(
a
)




































































(
b
)






























































(
c
)

F
i
g
.

3

E
l
e
m
e
n
t
a
l

m
a
p
s

s
h
o
w
i
n
g

t
h
e

d
i
s
t
r
i
b
u
t
i
o
n

o
f

C
o
,

C
r
,

N
i
,

F
e
,

a
n
d

C

i
n

(
a
)

0

w
t
.
%

c
h
r
o
m
i
u
m

c
a
r
b
i
d
e
,

(
b
)

1
0

w
t
.
%

c
h
r
o
m
i
u
m

c
a
r
b
i
d
e

a
n
d
(
c
)

2
0

w
t
.
%

c
h
r
o
m
i
u
m

c
a
r
b
i
d
e

c
o
a
t
i
n
g
s
.

F
e
C
F
e
F
e
C
C
3
a
-
5
3

a
-
6
3

b
-
6

3

c
-
6
3

b
-
5

3
c
-
5
A
r
e
a

A
r
e
a

24
4 0 5 0 6 0 7 0 8 0 9 0 1 0 0
6 0
8 0
1 0 0
1 2 0
1 4 0
1 6 0
Fig. 4 XRD spectrum showing various phases in 0 wt.% chromium carbide coating.
4 0 5 0 6 0 7 0 8 0 9 0 1 0 0
4 0
6 0
8 0
1 0 0
1 2 0
1 4 0
1 6 0
1 8 0
Fig. 5 XRD spectrum showing various phases in 10wt.% chromium carbide coating.
4 0 5 0 6 0 7 0 8 0 9 0 1 0 0
6 0
8 0
1 0 0
1 2 0
1 4 0
1 6 0
1 8 0
2 0 0
2 2 0


Fig. 6 XRD spectrum showing various phases in 20wt.% chromium carbide coating
1- Ni-Cr-Fe-C
1, 3,5, 6
2- M23C6
1, 2, 3 2
3- Ni4W
4
4- CoWSi
4
6- Fe2O3
7
5
6
5- Fe3C 7- NiO2
8- Cr2O3
5
8
7
8
5- FeNi3 1- Cr23C6 2- Cr7C3 3- Co7W6 4- WSi2
1, 2, 3, 4,
1, 2, 5
3
1
4
1
1
1
1, 2, 3, 4
1- Cr7C3 2- Co3 W9 C4 3- Ni31 Si12 5- FeNi3 4- Fe3C
3, 5
1
2
1
5
4
R
e
l
a
t
i
v
e

I
n
t
e
n
s
i
t
y
Diffraction angle 2
R
e
l
a
t
i
v
e

I
n
t
e
n
s
i
t
y
R
e
l
a
t
i
v
e

I
n
t
e
n
s
i
t
y
Diffraction angle 2
Diffraction angle 2
25
640
660
680
700
720
740
760
780
800
0 wt.% 10 wt.% 20 wt.%
V
i
c
k
e
r
s

h
a
r
d
n
e
s
s

(
H
v

5
)
Wt.% Chromium carbide
0
1
2
3
4
5
6
7
8
9
10
0 wt.% 10 wt.% 20 wt.%
P
o
r
o
s
i
t
y

(
%
)
Wt.% Chromium carbide


Fig. 7 Effect of chromium carbide addition in 1006-20wt.%WC powder coating
on (a) hardness (Hv
5
) and (b) porosity (%).



0.00 5.00 10.00 15.00 20.00
0.0028
0.0281
0.0534
0.0787
0.104
a
Composition (C), wt.%CrC
A
b
r
a
s
i
v
e

w
e
a
r
,

g

:
25.00 40.00 55.00 70.00 85.00
0.0028
0.0281
0.0534
0.0787
0.104
d
Sliding Distance (S), m
A
b
r
a
s
i
v
e

w
e
a
r
,

g

20.00 40.00 60.00 80.00 100.00
0.0000
0.0153
0.0306
0.0459
0.0612
c
Abrasive size (A), m
A
b
r
a
s
i
v
e

w
e
a
r
,

g

5.00 10.00 15.00 20.00 25.00
-0.0005
0.0150
0.0304
0.0458
0.0612
Load (L), N
b
A
b
r
a
s
i
v
e

w
e
a
r
,

g

69686
74195
786112
a b
7.7
8.6
9.2
26
Fig. 8 Effects of individual factors such as (a) %CrC-concentration (C), (b) load (L), (c)
abrasive size (A) (d) sliding distance (S) and (e) temperature (T) on abrasive
wear.

50.00 75.00 100.00 125.00 150.00
0.0028
0.0281
0.0534
0.0787
0.104
e
Temperature (T), C
A
b
r
a
s
i
v
e

w
e
a
r
,

g

0.0000
0.0153
0.0306
0.0459
0.0612
0.00
5.00
10.00
15.00
20.00
5.00
10.00
15.00
20.00
25.00
a
A
b
r
a
s
i
v
e

w
e
a
r
,

g

Load (L), N
0.0000
0.0153
0.0306
0.0459
0.0612
0.00
5.00
10.00
15.00
20.00
50.00
75.00
100.00
125.00
150.00
b
A
b
r
a
s
i
v
e

w
e
a
r
,

g

Temperature
(T), C
Composition (C),
wt.%CrC
Composition (C),
wt.%CrC
27

Fig. 9 Effects of interactions (a) composition-load (CL), (b) composition-temperature
(CT), (c) load-abrasive size (LA), (d) load-sliding distance (LS) and (e) abrasive
size and-sliding distance (AS) on abrasive wear.
0.0000
0.0153
0.0306
0.0459
0.0612
5.00
10.00
15.00
20.00
25.00
20.00
40.00
60.00
80.00
100.00
c
A
b
r
a
s
i
v
e

w
e
a
r
,

g

Abrasive size
(A), m
0.0000
0.0153
0.0306
0.0459
0.0612
5.00
10.00
15.00
20.00
25.00
25.00
40.00
55.00
70.00
85.00
d
A
b
r
a
s
i
v
e

w
e
a
r
,

g

Sliding Distance
(S), m
0.0000
0.0153
0.0306
0.0459
0.0612
20.00
40.00
60.00
80.00
100.00
25.00
40.00
55.00
70.00
85.00
e
A
b
r
a
s
i
v
e

w
e
a
r
,

g

Sliding Distance
(S), m
Load (L), N
Load (L), N
Abrasive size
(A), m
28

Fig.10 SEM micrographs of worn surfaces (a) 0%wt. chromium carbide, (b) 10%wt. chromium
carbide .
b
Cutting
a
Ploughing
Sliding Direction